Chemical Mapping of Silica Prepared via Sol-Gel Reaction in Rubber Nanocomposites
Chemical Mapping of Silica Prepared via Sol-Gel Reaction in Rubber Nanocomposites
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DOI：
10.1021/ma5020929
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发表时间：
2015-01
期刊：
影响因子：
5.5
通讯作者：
E. Miloskovska;Cornelius Friedrichs;D. Hristova-Bogaerds;Olivier Persenair;M. Duin;M. Hansen
中科院分区：
文献类型：
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作者：
E. Miloskovska;Cornelius Friedrichs;D. Hristova-Bogaerds;Olivier Persenair;M. Duin;M. Hansen
以天然橡胶和三元乙丙橡胶为基体，正己基胺为催化剂，采用原位水解缩合法制备了含10wt%二氧化硅的橡胶-二氧化硅纳米复合材料。溶胶-凝胶合成的二氧化硅的结构，映射由固态NMR光谱和XPS，表明残留的乙氧基基团的存在下，内部的二氧化硅颗粒和二氧化硅表面上，而己胺优先驻留在二氧化硅表面稳定通过氢键的乙氧基和化学吸附的己胺。因此，溶胶-凝胶合成的二氧化硅的制备导致形成具有增加的疏水性质的所谓的“毛状”二氧化硅颗粒。组合技术FTIR-TGA-MS证实了溶胶-凝胶合成二氧化硅的复杂化学性质以及颗粒和原位橡胶-二氧化硅纳米复合材料中存在少量残留乙醇，后一方面很重要..
Rubber–silica nanocomposites containing 10 wt % silica were prepared using in situ hydrolysis and condensation of tetraethyl orthosilicate (TEOS) in the presence of n-hexylamine as catalyst in two rubber matrices, namely, natural rubber and ethylene-propylene diene rubber. The structure of sol–gel synthesized silica, mapped by solid-state NMR spectroscopy and XPS, indicated the presence of remnant ethoxy groups inside the silica particles and on the silica surface, while hexylamine resided preferentially at the silica surface stabilized via hydrogen bonding of the ethoxy and chemisorption of the hexylamine. Thus, the preparation of sol–gel synthesized silica results in the formation of so-called “hairy” silica particles with increased hydrophobic properties. The combinatory technique FTIR-TGA-MS confirms the complex chemistry of the sol–gel synthesized silica as well as the low amount of residual ethanol present in the particles and the in situ rubber–silica nanocomposite, the latter aspect being importan...